IRT 5000/7000 Infrared Microscopes JASCO Pr oduc t Se minar e b 9 - - PowerPoint PPT Presentation

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IRT 5000/7000 Infrared Microscopes JASCO Pr oduc t Se minar e b 9 - - PowerPoint PPT Presentation

IRT 5000/7000 Infrared Microscopes JASCO Pr oduc t Se minar e b 9 th 2018, Kuala L F umpur Contents Basic of Infrared Microspectrometry Advantage of IRT-5000/7000 Competitive information Basic of Infrared Microspectrometry


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JASCO Pr

  • duc t Se minar

F e b 9th 2018, Kuala L umpur

IRT‐5000/7000

Infrared Microscopes

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Contents ・Basic of Infrared Microspectrometry ・Advantage of IRT-5000/7000 ・Competitive information

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Basic of Infrared Microspectrometry

・Target – Micro object Sample size : micron order ・Mapping measurement for small area, or analysis of change state by heating/cooling. ・The result is local information of micron area. Spectrum may be changed when you change the measurement position. The material seems to be ununiform, several points should be measured

  • -> Mapping / Imaging analysis is needed

Analysis by microscopic measurement

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IR microscope measurement

Transmission Refrection ATR Type of measurement Sample Minimun size Sample Thickness

x 32 : 5x5 um x 16 : 10x10 um 10x10 um 0.1 – 10 um 0.1 – 5 um Doesn’t matter 0.1um -

RAS

100x100 um Several 10 Å – 0.1 um x 32 : 10x10 um x 16 : 20x20 um

Standard mid-band MCT detector Please note that these specification may be changed according to sample !

Basic of Infrared Microspectrometry

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[ Target sample and measurement method] ・Foreign material, in powdery form

  • > Pick up it and make KBr plate, Transmission method.

・Foreign material on the Electronic substrate, Camera lens, micro relay switch

  • > If you pick it up, Transmission method.

Difficult to pick up, and metal base plate (IR light reflection), Reflection method. and resin base plate (smooth surface), ATR method. ・Contamination in medicine and food

  • > Pick up and Transmission method, or if it is on the surface
  • f the sample, ATR method.

・Thin layer film, thinner than 0.1um, on the metal plate or very thin film form.

  • > Reflection absorption spectroscopy, RAS method.

Basic of Infrared Microspectrometry

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Advantage of IRT-5000/7000

FT/IR main unit Light source, Interferometer IR microscope (IRT-5000 series) Microscope optica system, Detector Control PC

IR microscope system

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Microscope measurement Standard model Wide area mapping measurement Wide area, high-speed mapping Wide area, high-speed, high resolution mapping IRT-5100 IRT-5200 IRT-7100 IRT-7200 Primary use 10μm2 1 Point Measurement OK OK OK OK Identification of foreign material IQ Mapping (320x320μm) × OK OK OK Mapping of foreign material and it’s peripheral, Separation of foreign material compound Wide Area Mapping (10x7.5cm) × OK OK OK Component distribution analysis High-speed Mapping (10data/sec) × × OK OK Scanning of whole sample Change of sample state High-speed, High resolution Mapping (160data/sec) × × × OK Scanning of microscopic material Time course mapping analysis

IRT-5100 IRT-5200 IRT-7100 IRT-7200

FT/IR Microscopes

Select instrument Depending on the purpose

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4 positions Revolver with various type of Cassegrain mirror

Transmission Reflection ATR RAS

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Slide Attachment and Auto Recognition

Example of ATR cassegrain installation (Slide-in)

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Cassegrain auto adjustment function

Auto focusing by IR light at measuement ! This is necessary for IR microscope !

Observation (Visible light focusing) Measurement (IR light focusing) Visible light IR light Sample

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Single action exchange of various type detector

Detector can be select as measurement purpose from 10 detectors. 2 detectors can be mounted on IR microscope, and one of them can be exchanged in a single operation.

Linear array midband MCT(7000-650)(1 x 16Element) Linear array midband MCT(7000-650)(2 x 16Element) Linear array InSbDetector(10000-1900) Linear array InGaAsDetector(10000-5000) Mid-band MCTDetector(7800-600) Narrow-band MCTDetector(7800-750) Wide-band MCTDetector(7800-450) DLATGSDetector(7800-400) InSbDetector(15000-1850) InGaAsDetector(12000-4000)

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DLATGS and MCT

Fig.1 New DLATGS and MCT, polystyrene film measurement

Measurement conditions FT/IR-6600 + IRT-5200 Aperture : 50 x 50um Accumulation : New DLATGS : x100 MCT : x50 Transmission method Accumulation number for DLATGS is twice as MCT, DLATGS have an ability to measure small area as 50x50um.

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IQ mapping

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Measurement method of IR microscope

1 point

  • Transmittance
  • Reflectance
  • ATR
  • RAS

Area

  • Transmittance
  • Reflectance
  • ATR
  • RAS

Specular reflectance Transmittance-reflectance Diffuse reflectance

Observation image 1649cm-1 Peak height

1.2 0.5 1 4000 750 1000 2000 3000 Abs Wavenumber [cm-1]

Mapping analysis

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Conventional method

1 point

  • Transmittance
  • Reflectance
  • ATR
  • RAS

Area

Specular reflectance Transmittance-reflectance Diffuse reflectance

Manual stage Auto stage

  • Transmittance
  • Reflectance
  • ATR
  • RAS

Mapping analysis Other manufacturer still classify analysis method as this category

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Conventional mapping and IQ mapping

Transmittance mapping by auto stage

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Conventional mapping and IQ mapping

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Conventional mapping and IQ mapping

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Conventional mapping and IQ mapping

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Conventional mapping and IQ mapping

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Conventional mapping and IQ mapping

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Conventional mapping and IQ mapping

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Conventional mapping and IQ mapping

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Conventional mapping and IQ mapping

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Conventional mapping and IQ mapping

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Measurement is completed !

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IQ mapping

1 point

  • Transmittance
  • Reflectance
  • ATR
  • RAS

Area

Specular reflectance Transmittance-reflectance Diffuse reflectance

Manual stage Auto stage

  • Transmittance
  • Reflectance
  • ATR
  • RAS

IQ Mapping

IQ mapping can cover all of the measurement method. Only Jasco can do this !

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Conventional mapping and IQ mapping

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Measurement is completed !

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IQ mapping

Advantage of mapping measurement A B C

Independently measure A, B and C data Mapping Image

A B C 1 point measurement by IR microscope

Data include all of the spectrum of A, B and C, it is not easy to analyze.

(macro) ATR measurement Mapping measurement by small aperture size Macro measurement (ATR) or 1 point measurement by IR microscope Mapping measurement by IR microscope A B C

Aperture (measurement unit) Aperture (measurement unit)

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Advantage of IR mapping measurement Data include multiple spectrum from multiple compounds, it is not easy to identify each compound. 1 point measurement

1 0.5 4000 650 2000 1000 Abs Wavenumber [cm‐1] 100 μm

Multi layer sample (white frame : measurement unit)

IQ mapping

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Mapping measurement

100 μm 100 μm

Multi layer sample (each white frame : measurement unit) Mapping Image

4000 650 2000 1000 Abs Wavenumber [cm‐1]

PVC + Protein PVC Polyester

0.5

Each component can be measured independently, then easily analyze it. Distribution of component is clear at a glance. Advantage of IR mapping measurement

IQ mapping

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Advantage of IQ mapping : Mapping measurement can be done without auto stage. Unique and epoch-making function. Only Jasco can do IQ mapping. Maximum mapping area by IQ mapping

Maximum mapping area, um

IQ mapping

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Clear View ATR

Clear View ATR, that overwhelms

  • ther manufacturers !

ATR-5000SD / SS

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ATR measurement Problems in other manufacturer

Problem 1 : Can not observe the sample surface

  • f contacting area of ATR prism

Nothing can be

  • bserved !

Observation Image

Can not perceive even if the measurement point is wrong !

Sample surface can not be

  • bserved when ATR prism is

contacted on it. Therefore, we don’t know precise measurement position by ATR. In particular, hard target sample

  • n the soft material (for ex.,

foreign material on the gel sample) will be slipped when the prism contact on it, as a result it is difficult to measure it.

Clear View ATR

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Clear View ATR + IQ mapping

ATR measurement Problems in other manufacturere

Problem 2 : measurement point is limited Only the center position of the prism can be measured.

Contamination

If you want to measure other place of the sample, once prism need to be detached from sample, move the sample position and contact the prism again. In this way, mapping data

  • f small sample or sticky

foreign material can not be measured.

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Observe and ATR measurement during contact

  • ATR for IR microscope, IRT-5000/7000
  • Both Observation and Measurement can

be done only by Clear View ATR

  • Sample observation is possible through

prism under the condition of contacting the prism onto sample.

  • IQ monitor & IQ mapping enables you to

measure desired position by ATR while

  • bserving the sample

IRT-5000+FT/IR-4100

Clear View ATR

Survey position : Observe and reflectance measurement ATR positon

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Clear Image by Clear View ATR

Before contact the prism (Survey position) After contact the prism (ATR position) Observation image by Clear View ATR before contact the prism (observation by cassegrain mirror) and after contact the prism onto sample. Contact surface is clearly seen.

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Clear View ATR and IQ monitor, IQ mapping

By combination of Clear View ATR and IQ monitor / IQ mapping, desired position can be freely measured in the state of contacting the prism onto sample and observing the sample. This feature is quite useful for the sample which is not possible to measure again (for example, sticky foreign sample). Plastic tape Paint

IR light

Sample

Prism contact on sample, and

  • bserving it, desired position can

be freely selected to measure. Only Jasco can offer this function.

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Measurement is completed !

Conventional mapping and IQ mapping : ATR

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

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Conventional mapping and IQ mapping : ATR

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Conventional mapping and IQ mapping : ATR

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Conventional mapping and IQ mapping : ATR

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Conventional mapping and IQ mapping : ATR

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Conventional mapping and IQ mapping : ATR

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Conventional mapping and IQ mapping : ATR

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Conventional mapping and IQ mapping : ATR

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Conventional mapping and IQ mapping : ATR

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Conventional mapping and IQ mapping : ATR

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Conventional mapping and IQ mapping : ATR

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Conventional mapping and IQ mapping : ATR

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Conventional mapping and IQ mapping : ATR

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Measurement is completed !

Conventional mapping and IQ mapping : ATR

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Measurement is completed !

Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Measurement is completed !

Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Measurement is completed !

Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Measurement is completed !

Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Measurement is completed !

Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Measurement is completed !

Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Measurement is completed !

Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Measurement is completed !

Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Measurement is completed !

Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Measurement is completed !

Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Measurement is completed !

Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Measurement is completed !

Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Measurement is completed !

Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Measurement is completed !

Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Measurement is completed !

Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Measurement is completed !

Conventional mapping and IQ mapping : ATR

ATR mapping by auto stage

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Measurement is completed !

Just One Time contacted + IQ mapping Faster measurement time, No need to worry about contamination

Measurement is completed ! Measurement is completed !

Conventional mapping and IQ mapping : ATR

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Clear View ATR : Analysis

Mapping Observation Image

50 um 20 um

<Conditions> Model : IRT-5000 Sample : Paint Resolution : 8cm-1 Accumulation :1 Method :ATR (ZnS) Area : 100x100 um2 (6x6 pixel)

0.5 0.1 0.2 0.3 0.4 4000 700 2000 1000 Abs Wavenumber [cm-1]

Oil-based parint Water-based paint

Mapping image can be obtain for high viscosity sample

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Conclusion of Clear View ATR

Real time sample observation is possible during contacting the prism onto sample. Measurement of interested position on the sample can be done while checking the observation image of the sample by real time observation and IQ mapping. Just One Time contacted + IQ mapping Faster measurement time, No need to worry about contamination

contacting of the prism onto sample

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User friendly software

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Microscope measurement window

Spectrum, Observation image, Measurement conditions etc., All information put in one window

Spectrum Real time display Measurement conditions Observation Image Thumbnail Real time data analysis

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Clearer Observation Image than Stereo Microscope

Stereo Microscope x20 objective lens x16 Cassegrain (zoom x1.0) IRT-5000/7000 series

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Auto Focus

Focus position 1 Focus position 2 Auto Focus graph Focus point

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Auto Brightness

After automatically adjusts brightness

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IQ monitor function

Observation Image, measurement position and Spectrum are shown in real time in one window.

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Spectrum recording function

Spectrum recording is suited to searching for a point where the spectrum of a sample with differing thickness is not saturated.

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Thumbnail

・ The window displayed on the microscopic image can be registered in the thumbnail. ・ The image registered in the thumbnail can be saved as linked with a spectrum. ・ The stage can be moved to the registered image position.

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Mapping data analysis by MCR

Each component of multi layer and foreign material on it is analyzed by IR imaging and MCR (Multivariate Curve Resolution) analysis

Component A

Main Component spectrum Observation image Mapping image Green:Protein,

Blue:PVC, Red:Polyester,Yellow:Polyethylene

Database search result of main component

Component B Component C Component D

Imaging analysis result of multi layer by MCR

Component A Component C Component B Component D Protein Polyester Polyethyl ene

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JASCO Sharing Holder

IR Microscope Raman Microscope The rotary sample holder will become a common standard.

JASCO Sharing Holder JASCO Sharing Holder

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Correction of the stage coordinate

NRS-4500 NRS-5500/7500 IRT-5200/7200

Coordinate origin Correction of coordinate

Register the coordinate origin by using certificated sample.

Certificated sample

Share (commonize) the coordinate between instrument

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IR microscope Observation image Raman microscope Observation image

Scanning image: Search the highly coincidence position. Select the comparison image

Position adjustment by image matching

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(1) Set the holder to IR microscope (2) IR measurement (3) Set the holder to Raman microscope (4) Position adjustment (5) Raman measurement (6) Analysis

IR Raman

IR Raman

Procedure

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Visible image Infrared chemical image

Cellulose PP PE PET 4000 1000 2000 3000 Wavenumber [cm-1]

  • Abs. (a. u.)

Cellulose PP PE PET

Raman chemical image

PP PE PET TiO

2

3000 500 1000 2000 Raman Shift [cm-1] PP PE PET TiO2

  • Int. (a. u.)

Example : Multi-layer film

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(1) PET + pigment (2) Cellulose + pigment

4000 1000 2000 3000 Abs Wavenumber [cm-1]

(2) Cellulose (1) PET (1) Organic pigment 1 (2) Organic pigment 2

2000 200 500 1000 1500 Raman Shift [cm-1]

  • a. u.

IR Raman

It is possible to analyze the material of the fiber and pigment by using IR spectroscopy with Raman spectroscopy together.

Measurement example of colored fiber

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  • It is possible to measure and analyze the same position
  • f the sample by using IR microscope and Raman

microscope.

  • JASCO can suggest the multiple analysis by IR

microscope and Raman microscope.

  • JASCO can supply easy and fast multiple analysis by

using JASCO Sharing Holder.

Summary of JASCO Sharing Holder